LiCoPO4 cathode from a CoHPO4·xH2O nanoplate precursor for high voltage Li-ion batteries
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Choi, Daiwon↗
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Results for “Scanning electron microscopy”
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Effect of supersonic spraying impact velocity on opto-electric properties of transparent conducting flexible films consisting of silver nanowire, ITO, and polyimide multilayers
We demonstrate the use of supersonic spraying for the deposition of silver nanowires (AgNWs) on a flexible polyimide (PI) substrate for the formation of transparent and conducting films (TCF) as an alternative to nonflexible ITO (indium tin oxide). The self-fused intersections of the NWs resulted in films with a low sheet resistance (Rs = 31 ..omega../sq) and fairly high transmittance (Tr = 92%) on a glass substrate. The effect of the impact speed of the supersonically sprayed AgNWs on the opto-electric properties of the flexible TCF was evaluated by varying the spray coating conditions. The fabricated films were characterized by X-ray diffraction analysis, atomic force microscopy, ultraviolet-visible spectroscopy, and scanning electron microscopy. Finally, cyclic bending tests were performed on the PI/AgNW films as well as PI/ZnO/indium tin oxide/AgNW films, and the changes in their electrical properties with bending were compared.
36 MATERIALS SCIENCE↗
Evaluation of post-weld heat treatments applied to FeCrAl alloy weldments
The nuclear incident at the Fukushima Daiichi nuclear power plant has created a strong push for accident-tolerant fuel cladding to replace current zirconium-based cladding. A current near-term focus on iron-chromium-aluminum (FeCrAl) alloys. Laser-welded FeCrAl samples (C35MN, C37M, and C35M10 TC) were subjected to three different post-weld heat treatment regimes: 650 °C for 5 h, 850 °C for 1 h, and 850 °C for 5 h. Here, the samples were then analyzed using optical light microscopy, micro-hardness indentation, and scanning electron microscopy coupled with energy-dispersive spectroscopy and electron backscatter diffraction. The base microstructure of C37M and C35M10 TC experienced significant grain coarsening outside the fusion zone due to the applied post-weld heat treatments, whereas Nb-rich precipitation in C35MN limited grain growth compared with the other alloys studied.
36 MATERIALS SCIENCE↗
Microstructures and mechanical properties of the welded AA5182/HC340LA joint by magnetic pulse welding
Highlights: • The magnetic pulse welding of 5× aluminum alloy with high strength steel is performed. • The microstructure evolution of welding interface under different parameters is investigated. • The intermediate layer is characterized by high-resolution transmission electron microscope and electron diffraction pattern. - Abstract: Magnetic pulse welding (MPW) is an innovative joining technology for dissimilar materials. The MPW with high joining qualities could be realized between high strength steel and 5× aluminum alloys. In this work, the MPW joints between aluminum alloy (AA 5182) sheet and high-strength low alloy steel (HC340LA) sheet were prepared under various discharge energies. The mechanical properties and microstructure observations were employed to evaluate the joint performance. Results showed that a lower discharge voltage tended to cause joints with poor quality. When the discharge energy increased, the failure position gradually changed from the weld zone to the weaker base metal (Al) during quasi-static tensile tests. In addition, the effect of discharge energies on microstructure evolution in the intermediate layer was revealed by high-resolution transmission electron microscopy (HRTEM) and scanning electron microscope (SEM). Atomic-scale diffusion was found to be the mainly welding mechanism of the Al/Fe joint. The intermetallic compound (IMC) FeAl{sub 2} and ultra-fine grains (UFG) were found in the intermediate layer under high discharge energy.
36 MATERIALS SCIENCE↗
Effect of equal channel angular pressing on the mechanical and tribological behavior of Al-Zn-Mg-Cu alloy
Highlights: • The correlation of microstructure, mechanical and wear properties has been studied. • The correlation between tensile properties and shear properties has been also studied. • Mechanical and tribological properties have been improved through the ECAP process of the Al-7075 alloy. • The dominant wear mechanisms in the initial material were adhesive and oxidative wear as well as delamination. • Abrasive and oxidative wear were the dominant wear mechanisms in ECAP processed specimens. - Abstract: Microstructure, mechanical properties and wear behavior of severely deformed Al-7075 alloy by equal channel angular pressing (ECAP) were studied. Microhardness, tensile and shear strength tests were performed to evaluate the mechanical properties of the material. The relationship between tensile and shear strength was also extracted. In addition, with the aim of study the wear behavior, the wear tests were performed by using a pin-on-disk machine under different normal loads. The microscopic observations i.e. transmission electron microscopy (TEM) and scanning electron microscope (SEM), were used to analyze the microstructure of specimens as well as the surface, subsurface and debris of worn specimens. Mechanical properties results showed that the hardness and strength (tensile and shear) of the ECAP-processed alloy were higher than that of the annealed alloy and increased with the increment of pass number. The wear test data revealed that the wear rate and friction coefficient decreased with increasing ECAP passes. The SEM analysis of worn specimens demonstrated that the dominant wear mechanisms of the annealed alloy were adhesion wear and delamination and the dominant wear mechanisms of ECAP processed alloy were abrasive wear and plowing bands. Oxidative wear was also observed at both annealed and ECAPed alloy. Totally, these results demonstrated that ultrafine-grained structure fabricated by ECAP, improves the wear resistance of the Al-7075 alloy.
36 MATERIALS SCIENCE↗
A strategy to eliminate selenium oxide islands formed on the ZnSe/GaAs epilayer
Atomically clean and smooth surfaces are essential for semiconductor device fabrication and epitaxial regrowth. In this regard, spontaneously formed oxide islands or clusters on the surfaces of II-VI semiconductor exposures to air can disrupt interface formation. Using ZnSe/GaAs heterostructures grown by molecular beam epitaxy (MBE), we investigated the effect of surface treatments in eliminating oxide islands. The samples were probed with atomic force microscopy, low-temperature photoluminescence, and scanning electron microscopy. Here, it was found that ultra-high vacuum (UHV) annealing at 200°C, regardless of annealing duration, largely removed the islands while leaving the crystallinity of the ZnSe and GaAs epilayers unaffected. UHV annealing at higher temperatures of 300°C completely removed the islands, but the optical properties of ZnSe and/or GaAs epilayers deteriorated depending on the annealing duration. Our observations provide guidance to set thermal annealing strategies for removing oxide islands from the surfaces of II-VI/III-V semiconductor heterostructures depending on the desired properties.
36 MATERIALS SCIENCE↗
Towards aging mechanisms of cross-linked polyethylene (XLPE) cable insulation materials in nuclear power plants
Cross-linked polyethylene (XLPE) cable insulation material undergoes simultaneous, accelerated thermal and gamma-radiation aging to simulate the long-term aging environment within nuclear power plants (NPPs). A variety of materials characterization tests, including scanning electron microscopy, thermo-gravimetric analysis, differential scanning calorimetry, oxidation induction time, gel-fraction and dielectric properties measurement, are conducted on pristine and differently aged XLPE samples. A preliminary model of one possible aging mechanism of XLPE cable insulation material under gamma radiation at elevated temperature of 115 °C is suggested.
accelerated aging↗
Quantifying and Qualifying Alloys Based on Level of Homogenization: A U-10Mo Alloy Case Study
Homogenization heat treatment is performed to attain uniformity in microstructure which is helpful to achieve the desired workability and microstructure in final products and, eventually, to gain predictive and consistent performance. Fabrication of low-enriched uranium alloys with 10 wt% molybdenum (U-10Mo) fuel plates involves multiple thermomechanical processing steps. It is well known that the molybdenum homogeneity in the final formed product affects the performance in the nuclear reactor. Here, to ensure uniform homogenization, a statistical method is proposed to quantify and characterize the molybdenum concentration variation in U-10Mo fuel plates by analyzing the molybdenum concentration measurement data from scanning electron microscopy energy dispersive spectroscopy line-scan. Statistical tolerance intervals (TI) are employed to determine the qualification of the U-10Mo fuel plate. We formulate an argument for the minimum number of independent samples to define fuel plate qualification if no molybdenum measurement data are available in advance and demonstrate that the given TI requirements can be equivalently reduced to a sample variance criterion in this application. The outcome of the statistical analysis can be used to optimize casting design and eventually increase productivity and reduce fabrication costs. The statistical strategy developed in this paper can be implemented for other applications especially in the field of material manufacturing to assess qualification requirements and monitor and improve the process design.
36 MATERIALS SCIENCE↗
Optical and electrical properties of silicon nanopillars
The electrical and optical properties of silicon nanopillars (Si NPs) are studied. Electron-beam lithography and reactive ion etching are used for the formation of ordered Si-NP arrays. The Si NPs with a diameter from 60 to 340 nm and a height from 218 to 685 nm are formed. The Si NPs are coated with a TiON{sup x} layer with a thickness of 8 nm for chemical and electrical passivation of the surface. Scanning electron microscopy and atomic-force microscopy are used to characterize the obtained structures. The Si-NP arrays acquire various colors when exposed to “bright-field” illumination. The spectra of reflection from the Si-NP arrays in the wavelength range 500–1150 nm are obtained.
36 MATERIALS SCIENCE↗
Influence of Realistic, Cyclic Atmospheric Cycles on the Pitting Corrosion of Austenitic Stainless Steels
Pitting corrosion was evaluated on stainless steels 304H, 304, and 316L the surfaces of which had ASTM seawater printed on them as a function of surface roughness after exposure to an exemplar realistic atmospheric diurnal cycle for up to one year. Methods to evaluate pitting damage included optical imaging, scanning electron microscopy imaging, profilometry analysis, and polarization scans. The developed cyclic exposure environment did not significantly influence pitting morphology nor depth in comparison to prior static exposure environments. Cross-hatching was observed in a majority of pits for all material compositions with the roughest surface finish (#4 finish) and in all surface finishes for the 304H composition. Evidence is provided that cross-hatched pit morphologies are caused by slip bands produced during the grinding process for the #4 finish or by material processing. Additionally, micro-cracking was observed in pits formed on samples with the #4 surface finish and was greatly reduced or absent for pits formed on samples with smooth surface finishes. This suggests that both a low RH leading to an MgCl 2 -dominated environment and a rough surface containing significant residual stress are necessary for micro-cracking. Finally, the use of various characterization techniques and cross sectioning was employed to both qualitatively and quantitatively assess pitting damage across all SS compositions and surface finishes.
36 MATERIALS SCIENCE↗
Core Characterization of Bakken Shale from the Bedwell 33-52-1-1H Well, Sheridan County, Montana
The computed tomography (CT) facilities and the Multi-Sensor Core Logger (MSCL) at the National Energy Technology Laboratory (NETL) in Morgantown, West Virginia were used to characterize core of the Bedwell 33-52-1-1H well (API 25-091-21920), a wildcat field in Sheridan County, Montana. The primary impetus of this work is to provide a unique dataset to researchers at universities, national laboratories, geological surveys, and other locations for additional analyses. The resultant datasets are presented in this report and can be accessed from NETL's Energy Data eXchange (EDX) online system using the following link: https://edx.netl.doe.gov/dataset/bedwell-33-52-1-1h-well. The equipment and techniques used to characterize the full core were non-destructive, enabling future examinations and analyses to be performed on these cores. However, none of the equipment used was suitable for direct visualization of the pore space in fine-grained structures such as those found in shales; fractures, discontinuities, and millimeter scale features were readily detectable with the methods tested. Imaging with the NETL medical CT scanner was performed on the entire core. Qualitative analysis of the medical CT images, coupled with X-ray fluorescence (XRF), P-wave, and magnetic susceptibility measurements from the MSCL were useful in identifying zones of interest for more detailed analysis. A selection of samples (Table 1) were cored, sliced, and powdered for additional characterization analyses. These analyses did involve destructive subsampling of the full core at discrete sections, and the results are presented here in the context of the larger core description. Selected sections of the core were removed from the full core for detailed analyses using the following destructive techniques: bulk inductively coupled plasma-optical emission spectroscopy (ICP-OES), isolation of carbon and sulfur, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and higher resolution CT scan with NETL’s micro-CT scanning systems. The ability to quickly identify key areas for more detailed study with higher resolution will save time and resources in future studies. The combination of methods used provides a multi-scale analysis of the core; the resulting macro and micro descriptions are relevant to many subsurface energy related examinations traditionally performed at NETL.
04 OIL SHALES AND TAR SANDS↗
Oxidation in oxygen at 900 deg and 1000 deg C of four nickel-base cast superalloys: NASA-TRW VIA, B-1900, alloy 713C, and IN-738
The oxidation at 900 and 1,000 C of four nickel-base superalloys in 1 atmosphere of slowly flowing oxygen was investigated. Thermogravimetric rate data were obtained for periods to 100 hours. The morphology and composition of the oxide scales formed after 100 hours were studied by optical microscopy, X-ray diffraction, electron microprobe, scanning electron microscopy, and X-ray photoelectron spectroscopy (ESCA). Alloys B-1900 and VIA were found to be primarily alumina formers, though probably 25 percent of their surface was covered by CR2O3-containing oxides at 900 C. Alloys 713C and IN-738 were primarily chromia formers, though the surface of 713C at 1,000 C was covered with NiO, and the surface of IN-738 at both temperatures was covered with a thin layer of TiO2.
Fryburg, G. C.↗
The effect of zirconium on the isothermal oxidation of nominal Ni-14Cr-24Al alloys
The isothermal oxidation of Ni-14Cr-24Al-xZr-type alloys was performed in still air at 1100, 1150, and 1200 C for times up to 200 hr. The zirconium content of the alloys varied from 0-0.63 atom percent (a/o). The oxidized surfaces were studied by optical microscopy, X-ray diffraction, and scanning electron microscopy. The base alloy was an alumina former with the zirconium-containing alloys also developing some ZrO2. The addition of zirconium above 0.066 a/o increased the rate of weight gain relative to the base alloy. Due to oxide penetratio, the weight gain increased with Zr content; however, the scale thickness did not increase. The Zr did increase the adherence of the oxide, particularly at 1200 C. The delta W/A vs. time data fit the parabolic model of oxidation. The specific diffusion mechanism operative could not be identified by analysis of the calculated activation energies. Measurements of the Al2O3 scale lattice constants yielded the same values for all alloys.
Kahn, A. S.↗
Process Developed for Generating Ceramic Interconnects With Low Sintering Temperatures for Solid Oxide Fuel Cells
Solid oxide fuel cells (SOFCs) have been considered as premium future power generation devices because they have demonstrated high energy-conversion efficiency, high power density, and extremely low pollution, and have the flexibility of using hydrocarbon fuel. The Solid-State Energy Conversion Alliance (SECA) initiative, supported by the U.S. Department of Energy and private industries, is leading the development and commercialization of SOFCs for low-cost stationary and automotive markets. The targeted power density for the initiative is rather low, so that the SECA SOFC can be operated at a relatively low temperature (approx. 700 C) and inexpensive metallic interconnects can be utilized in the SOFC stack. As only NASA can, the agency is investigating SOFCs for aerospace applications. Considerable high power density is required for the applications. As a result, the NASA SOFC will be operated at a high temperature (approx. 900 C) and ceramic interconnects will be employed. Lanthanum chromite-based materials have emerged as a leading candidate for the ceramic interconnects. The interconnects are expected to co-sinter with zirconia electrolyte to mitigate the interface electric resistance and to simplify the processing procedure. Lanthanum chromites made by the traditional method are sintered at 1500 C or above. They react with zirconia electrolytes (which typically sinter between 1300 and 1400 C) at the sintering temperature of lanthanum chromites. It has been envisioned that lanthanum chromites with lower sintering temperatures can be co-fired with zirconia electrolyte. Nonstoichiometric lanthanum chromites can be sintered at lower temperatures, but they are unstable and react with zirconia electrolyte during co-sintering. NASA Glenn Research Center s Ceramics Branch investigated a glycine nitrate process to generate fine powder of the lanthanum-chromite-based materials. By simultaneously doping calcium on the lanthanum site, and cobalt and aluminum on the chromium site, we could sinter the materials below 1400 C. The doping concentrations were adjusted so that the thermal expansion coefficient matched that of the zirconia electrolyte. Also, the investigation was focused on stoichiometric compositions so that the materials would have better stability. Co-sintering and chemical compatibility with zirconia electrolyte were examined by X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy (line scanning and dot map). The results showed that the materials bond well, but do not react, with zirconia electrolyte. The electric conductivity of the materials measured at 900 C in air was about 20 S/cm.
Zhong, Zhi-Min↗
Observations of Screw Dislocation Driven Growth and Faceting During CVD Homoepitaxy on 4H-SiC On-Axis Mesa Arrays
Previous studies of (0001) homoepitaxial growth carried out on arrays of small-area mesas etched into on-axis silicon-face 4H-SiC wafers have demonstrated that spiral growth emanating from at least one screw dislocation threading the mesa is necessary in order for a mesa to grow taller in the <0001> (c-axis vertical) direction while maintaining 4H stacking sequence [1]. However, even amongst mesas containing the screw dislocation step source necessary for vertical c-axis growth, we have observed striking differences in the height and faceting that evolve during prolonged homoepitaxial growths. This paper summarizes Atomic Force Microscopy (AFM), Electron Channeling Contrast Imaging (ECCI), Scanning Electron Microscopy (SEM), and optical microscopy observations of this phenomenon. These observations support our initially proposed model [2] that the observed large variation (for mesas where 3C-SiC nucleation has not occurred) is related to the lateral positioning of a screw dislocation step source within each etched mesa. When the screw dislocation step source is located close enough to the developing edge/sidewall facet of a mesa, the c-axis growth rate and facet angle are affected by the resulting interaction. In particular, the intersection (or near intersection) of the inward-sloping mesa sidewall facet with the screw dislocation appears to impede the rate at which the spiral provides new steps required for c-axis growth. Also, the inward slope of the sidewall facet during growth (relative to other sidewalls of the same mesa not near the screw dislocation) seems to be impeded by the screw dislocation. In contrast, mesas whose screw dislocations are centrally located grow vertically, but inward sloping sidewall facets shrink the area of the top (0001) growth surface almost to the point of vanishing.
Neudeck, Philip G.↗
Corrosion Behavior of Plasma-Nitrided 904L Austenitic Stainless Steel in Hydrofluoric Acid
A new type of high-chromium nickel molybdenum super austenitic stainless steel, 904L, has excellent corrosion resistance in acidic environments. However, the service life of 904L decreases significantly in a mixed acid system that includes hydrogen fluoride and sulfuric acid. In this article, different plasma nitriding processes were used to modify the surface of 904L stainless steel. X-ray diffraction was used to analyze the phase composition after nitriding; scanning electron microscopy and atomic force microscopy were used to examine the surface morphology after nitriding; electrochemical noise and electrochemical methods were used to study the localized corrosion behavior and the damage mechanism of the ion nitride layer; and the effect of the plasma nitride layer on the corrosion resistance was explored. The results show that with increasing nitriding time, the thickness of the nitride layer increased. Ion nitriding resulted in the coarsening of the 904L austenitic stainless steel surface. A long nitriding treatment time resulted in the precipitation of CrN in the modified layer, depleting the chromium from the matrix and remarkably reducing the corrosion resistance.
36 MATERIALS SCIENCE↗
Regular Microstructures Based on Polyethylene Terephthalate Films
A method for forming regular dielectric and metallic microstructures based on polyethylene terephthalate films irradiated with a synchrotron radiation source through a mask with subsequent etching. To study their geometric parameters, scanning electron microscopy was used.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
Influence of MnC{sub 2}O{sub 4} microadditives on combustion characteristics of CuO/Al nanoenergetics
In this work, we have investigated the catalytic effect of MnC{sub 2}O{sub 4} microrods on combustion characteristics of CuO/nAl nanoenergetic composites. CuO nanorods were prepared by solid state synthesis method using the nonionic surfactant of poly(ethylene)glycol of molecular weight 400 (PEG400). The crystal information and microstructure of CuO/nAl nanoenergetics were studied by X-ray diffractometry and Transmission Electron microscopy. Microrods shaped manganese oxalate (MnC{sub 2}O{sub 4}) were fabricated by using mild thermal precipitation and aging process and confirmed by energy dispersive X-ray spectroscopy (EDS). The microstructures of MnC{sub 2}O{sub 4} microrods and the nanoenergetic composites of CuO/nAl/MnC{sub 2}O{sub 4} were characterized by Field emission scanning electron microscopy (FE-SEM) imaging. The addition of MnC{sub 2}O{sub 4} microrods has demonstrated a significant enhancement in dynamic pressure-time characteristics of CuO/nAl nanoenergetics.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗